Classifications

• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
  • B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
  • B02C19/00—Other disintegrating devices or methods
  • B02C19/08—Pestle and mortar
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
  • B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
  • B02C13/00—Disintegrating by mills having rotary beater elements ; Hammer mills
  • B02C13/02—Disintegrating by mills having rotary beater elements ; Hammer mills with horizontal rotor shaft
  • B02C13/06—Disintegrating by mills having rotary beater elements ; Hammer mills with horizontal rotor shaft with beaters rigidly connected to the rotor
  • B02C13/09—Disintegrating by mills having rotary beater elements ; Hammer mills with horizontal rotor shaft with beaters rigidly connected to the rotor and throwing the material against an anvil or impact plate
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
  • B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
  • B02C1/00—Crushing or disintegrating by reciprocating members
  • B02C1/02—Jaw crushers or pulverisers
  • B02C1/025—Jaw clearance or overload control
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
  • B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
  • B02C1/00—Crushing or disintegrating by reciprocating members
  • B02C1/14—Stamping mills
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
  • B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
  • B02C25/00—Control arrangements specially adapted for crushing or disintegrating
• • C—CHEMISTRY; METALLURGY
  • C01—INORGANIC CHEMISTRY
  • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
  • C01B33/00—Silicon; Compounds thereof
  • C01B33/02—Silicon
• • C—CHEMISTRY; METALLURGY
  • C01—INORGANIC CHEMISTRY
  • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
  • C01B33/00—Silicon; Compounds thereof
  • C01B33/02—Silicon
  • C01B33/021—Preparation
  • C01B33/027—Preparation by decomposition or reduction of gaseous or vaporised silicon compounds other than silica or silica-containing material
  • C01B33/035—Preparation by decomposition or reduction of gaseous or vaporised silicon compounds other than silica or silica-containing material by decomposition or reduction of gaseous or vaporised silicon compounds in the presence of heated filaments of silicon, carbon or a refractory metal, e.g. tantalum or tungsten, or in the presence of heated silicon rods on which the formed silicon is deposited, a silicon rod being obtained, e.g. Siemens process

Definitions

• the invention relates to an apparatus and a method for comminuting polycrystalline silicon.
• Polycrystalline silicon is obtained by thermal decomposition of silicon compounds, such as trichlorosilane, in a so-called. Siemens reactor and thereby accumulates in the form of polycrystalline rods.
• the polycrystalline rods To produce single crystals by means of crucible pulling, the polycrystalline rods must first be broken up into fragments. Also for applications in the solar industry, the grown polycrystalline rods must first be crushed into fragments.
• US 5,660,335 A discloses a crushing process in which a high pressure water jet is shot at a crystal rod.
• US 2010/025060 A1 describes a breaking tool comprising a pneumatic piston driving means for urging the piston installed in a housing from a retreating position to a projection position by air pressure, a guide tube connected to the housing and extending in the direction of movement of the piston, and a hammer head.
• the rear end portion of the hammer head is movably inserted in the front end portion of the guide tube.
• the piston When the piston is moved from the retracted position to the projecting position, the front end of the piston collides with the rear end of the hammer head.
• US 7,360,727 B2 discloses a mechanical crusher for crushing a polycrystalline silicon rod, comprising a backing and crushing bits and counter-bits, wherein crushing bits and counter-bits have a longitudinal axis aligned at right angles to the longitudinal axis of the backing and parallel to the surface of the backing, and the shredding bit and counter-chisel are so movable in that a silicon rod to be comminuted on the surface of the base can be adjusted between the bits in such a way that all the bits in the area of the silicon rod are in contact with the silicon rod and the comminution chisels in front of and behind the silicon rod are moved in the direction of their longitudinal axis to a safety distance to the counter-chisel can be and affect the crushing bits by means of a shock-shaped movement in the direction of its longitudinal axis on the silicon rod and smash it.
• US 7,360,727 B2 a method for mechanical comminution of a polycrystalline silicon rod, wherein the polycrystalline silicon rod is on a height-adjustable support and is adjusted there between comminution and counter-chisel such that all chisels in the region of the silicon rod contact the silicon rod and crushing chisel and counter-chisel in front of or behind the silicon rod be approximated to a safety distance and then a recurring impact pulse is started at all abutting the silicon rod crushing chisels, which causes a comminution of the silicon rod.
• US 2011/068206 A1 describes a crusher for efficiently crushing a silicon lump, whereby little fine breaking material (powder) is formed.
• the breaking tool comprises a hammer head connected to a piston, the hammer head being in a rest position without compressed air and being moved by the application of compressed air from the rest position to collide with a silicon lump.
• In the crusher is a plurality of spaced-apart crushing tools, each with a hammer head opposite the silicon lumps located on a base.
• a device for comminuting a polycrystalline silicon rod comprising a base and at least one movable comminution tool and at least one immovable anvil, wherein the at least one comminution tool has a longitudinal axis which is aligned parallel or nearly parallel to the surface of the substrate lying on the surface of the pad, to be comminuted silicon rod between the shredder chisel and anvil can be adjusted so that crushing chisel and anvil can each have in the region of the silicon rod contact with the silicon rod and one contact point of silicon rod and anvil and extending through a rod center transverse axis of the Silicon rod or a parallel to that transverse axis and up to 30% of a rod diameter from the rod center spaced axis of the silicon rod on the Longitudinal axis of the comminution chisel or on a parallel to the longitudinal axis of the comminution chisel and spaced by up to 30% of the rod diameter of the
• the object of the invention is also achieved by a method for comminuting a polycrystalline silicon rod, in which the polycrystalline silicon rod is located on a base and is adjusted there between at least one movable comminution tool and at least one immovable anvil such that comminution chisel and anvil respectively in the Silicon rod can have contact with the silicon rod and a contact point of silicon rod and anvil and extending through a rod center transverse axis of the silicon rod or parallel to that transverse axis and up to 30% of a rod diameter from the rod center axis of the silicon rod on the longitudinal axis of the comminution chisel or on a parallel to the longitudinal axis of the comminution chisel and spaced by up to 30% of the rod diameter of the longitudinal axis of the comminution chisel axis, and then a shock pulse is started, wherein at m Start the impact pulse Do not touch the chisel and silicon rod, the comminution
• the silicon rod is preferably a largely rotationally symmetrical body with a substantially circular cross section, which comprises a longitudinal axis and a transverse axis.
• a transverse axis of the silicon rod passing through a rod center or parallel to that transverse axis is up to 30%.
• both anvils and comminution bits may be independently displaced up to 30% in either direction from the transverse axis of the silicon rod passing through a bar center.
• the transverse axis of the silicon rod lying parallel to the longitudinal axis of the comminution tool or on an axis parallel to the longitudinal axis of the comminution tool and spaced up to 30% of the rod diameter from the longitudinal axis of the comminution tool is up to 10% of the rod diameter from the transverse axis of the rod center Staff removed.
• the transverse axis of the silicon rod parallel to the longitudinal axis of the comminution tool or parallel to the longitudinal axis of the comminution tool and spaced up to 10% of the rod diameter from the longitudinal axis of the comminution tool is up to 30% of the rod diameter from the transverse axis of the rod center Staff removed.
• the transverse axis of the silicon rod lying on the longitudinal axis of the comminution tool or on a transverse axis parallel to the longitudinal axis of the comminution tool and spaced by up to 10% of the rod diameter from the longitudinal axis of the comminution tool to 10% of the rod diameter from the transverse axis of the rod passing through the rod center.
• the transverse axis of the silicon rod passing through the rod center and the longitudinal axis of the comminution tool and the abutment point between the anvil and silicon rod lie on a common axis, in other words, the contact point between the anvil and silicon rod and rod center of the silicon rod lie on the longitudinal axis of the comminution tool.
• the rod center of the silicon rod is a point on the geometric axis (center of gravity axis, which connects the cross-sectional centers of gravity) of the cylindrical rod to understand.
• An attachment point is a point of contact between anvil and silicon rod.
• the comminuting bit is movable and can preferably be moved in two directions parallel to the direction of impact and perpendicular to the plane of the base to compensate for differences in diameter of the silicon rods.
• the entire crushing unit comprising a plurality of shredding bits is designed to be movable.
• the base parallel to the direction of impact and perpendicular to the plane of the base, the base could itself be designed to be movable in the same way for the movement of the comminution chisel.
• the comminution chisel is preferably aligned parallel or up to 30 ° inclined to the base. Particularly preferred is an inclination of the comminution chisel of 10 °, in the ideal case comminution chisel and base are arranged in parallel.
• an opposed anvil is provided, which is immovable relative to the base and preferably has the shape of a cylinder or a semi-cylinder.
• the cylindrical shape should also Include components with an elliptical or semi-elliptical cross section.
• the surface of the anvil that comes in contact with the silicon rod should always be curved. This shape can ensure that the silicon rod with the anvil has exactly one contact point or contact point.
• the anvil can be constructed in one piece and in several parts. Also, the multi-part construction of the anvil should be designed so that there is exactly one point of contact between anvil and silicon rod.
• anvil during operation, that are triggered during beat pulses, immobile and rigidly fixed.
• the anvils may well be designed to be movable to facilitate anvil, silicon rod and comminution chisel adjustment.
• the geometric axis of the anvil is preferably perpendicular or nearly perpendicular to the impact axis.
• the geometric axis of the anvil can be inclined by up to 30 ° against the striking axis. Particularly preferred is an inclination of the anvil of 10 °, ideally, the geometric axis of the anvil and the axis of impact are perpendicular to each other.
• the impact axis is given by the longitudinal axis of the comminution chisel.
• One end of the comminution chisel, which comes into contact with the silicon rod, preferably has a round shape and preferably does not comprise a flattening.
• a distance of the end of the comminution chisel to the silicon rod is preferably chosen so that it corresponds to the preset stroke of the comminution chisel minus the possible penetration into the silicon rod corresponds.
• Hub is a preset linear movement of the comminution chisel towards the workpiece.
• the stroke can usually be varied by adjustable stops. The larger the stroke, the higher the impact energy.
• the anvils are preferably rigidly fixed during operation.
• the impact axis or longitudinal axis of the at least one comminution chisel and base are preferably inclined at an angle of 0-90 ° to the horizontal.
• the silicon rod contacts the pad (which in this case is a lateral boundary of the device) and rests on the anvil.
• Particularly preferred is an inclination angle of 1-45 °, so that a lying on the base silicon rod rolls by its own weight against the at least one anvil.
• Very particularly preferred is an inclination angle of 1-20 °.
• Anvil (s) and the end (s) of comminution chisel (s) are preferably made of tungsten carbide (WC).
• WC tungsten carbide
• carbide coated steels or ceramics may be used for the anvil (s) and end (s) of comminution chisel (s).
• a beating sequence over the length of a silicon rod is preferably carried out alternately from outside to inside.
• a shock pulse is carried out by one of the outer comminution chisel, then a shock pulse through the present on the other side of the length of the silicon rod crushing chisel, and then alternately impact pulses through the further inside comminution chisel.
• These alternating beats are preferably carried out in a comparatively short time interval of 5-1000 ms.
• To avoid the influence of neighboring chisels and thus To increase the service life of the chisel is preferably reduced again after each blow and before triggering the follower chisel of the predecessor chisel.
• the different areas of a comminution chisel row can be divided into groups to run the impact sequences in all groups in parallel.
• the inventors have recognized by a variety of crushing experiments that optimum fracture result with the lowest possible impact energy can be achieved only if one investment point of silicon rod and anvil and extending through a rod center transverse axis of the silicon rod or parallel to that transverse axis and to axis of the silicon rod spaced 30% of a rod diameter from the rod center on the longitudinal axis of the comminution tool or on an axis parallel to the longitudinal axis of the comminution tool and spaced up to 30% of the rod diameter from the longitudinal axis of the comminution tool. It was also investigated how different silicon material behaves. These were experiments with slightly brittle, porous material and with compact silicon carried out. The stiffness of the anvils was also varied in the experiments.
• slightly brittle material With slightly brittle material, the design of the anvil has less influence on the fracture behavior. Irrespective of the design of the anvil, about 75 J is sufficient to crush such a rod. With slightly brittle material can be completely dispensed with an anvil, as previously mentioned.
• an impact energy of 400 J is sufficient if a hard and rigidly fixed anvil is used.
• this is an anvil made of tungsten carbide, which is fixed by a solid, rigid frame construction. If instead an anvil made of a softer, yielding material is used or a resilient frame construction is used to fix the anvil, an impact energy of at least 1000 J is necessary to smash a compact rod.
• low impact energy reduces the contamination input to the polycrystalline silicon.
• the optimal fracture arrangement which provides for the impact axis to be parallel to the substrate, minimizes the load on the substrate during fracture.
• the pad may be made of materials that are less harmful to contamination of the silicon. These are, for example, silicon, PU or other plastics.
• the preferred elongated cylindrical shape of the anvil allows the entire coverage of the bar diameter to be broken.
• the height of the anvil above the base is preferably to be chosen so that it corresponds to at least half the diameter of the rod.
• the single impact method reduces the contamination input by contact with the comminution chisel and anvil compared to a repeating impact pulse proposed in the prior art.
• the anvil as a contact point should ideally be hard and rigidly fixed in order to optimally reflect the impact pulse.
• a movable by moving teeth counter-bit - as claimed in the prior art - can not fulfill this task.
• An impact sequence which takes place alternately from the rod ends ultimately to the middle of the bar, effectively prevents changes in position of the rod (without an otherwise necessary lateral clamping or stop).
• the device and the method can be provided to dispense with anvils.
• the striking axis and base are horizontal in this case. If the required energy of fracture in the range ⁇ 400 J moves, easily brittle silicon rods can be broken even without anvil. This eliminates the risk of contamination by contact with the carbide anvils.
• the lining of the pad can be provided with low-contamination materials (silicon, PU, plastics) at a sufficient distance from the fracture zone. To stabilize the rod, a suitable recess may be provided in the pad.

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• Engineering & Computer Science (AREA)
• Chemical & Material Sciences (AREA)
• Organic Chemistry (AREA)
• Food Science & Technology (AREA)
• Mechanical Engineering (AREA)
• Inorganic Chemistry (AREA)
• Silicon Compounds (AREA)
• Crushing And Grinding (AREA)
• Crushing And Pulverization Processes (AREA)

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• 2012
  • 2012-08-01 DE DE102012213565.0A patent/DE102012213565A1/de not_active Withdrawn
• 2013
  • 2013-06-20 CA CA2820474A patent/CA2820474C/fr not_active Expired - Fee Related
  • 2013-06-26 TW TW102122685A patent/TWI522175B/zh active
  • 2013-07-04 ES ES13175097.8T patent/ES2558173T3/es active Active
  • 2013-07-04 EP EP13175097.8A patent/EP2692441B1/fr active Active
  • 2013-07-08 US US13/936,292 patent/US9586210B2/en active Active
  • 2013-07-17 KR KR1020130083895A patent/KR20140017430A/ko not_active Application Discontinuation
  • 2013-07-31 CN CN201310328379.4A patent/CN103567040B/zh active Active
  • 2013-07-31 JP JP2013159386A patent/JP5763136B2/ja active Active

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